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Colorimetric-fluorescent dual-channel recognition of mercury ion acceptor compound and its preparation and application

A compound, mercury ion technology, applied in the field of cation detection, can solve the problems of inability to meet the needs of cheap and fast on-site detection, low sensitivity, and failure to reach the limit value.

Inactive Publication Date: 2015-12-09
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, most of the mature mercury detection technologies rely on large-scale analytical instruments, which cannot meet the needs of cheap and fast on-site detection.
However, commercialized rapid detection instruments and mercury test strips have low sensitivity (the lower limit of detection is 0.1mg / L), which cannot reach the limits stipulated by the national standard (0.05mg / L for sewage, 0.001mg / L for drinking water), and Poor selectivity, unable to meet sensitive and accurate detection requirements

Method used

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  • Colorimetric-fluorescent dual-channel recognition of mercury ion acceptor compound and its preparation and application
  • Colorimetric-fluorescent dual-channel recognition of mercury ion acceptor compound and its preparation and application
  • Colorimetric-fluorescent dual-channel recognition of mercury ion acceptor compound and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1. Synthesis of receptor compounds

[0040] (1) Synthesis of intermediate 5-(nitrophenyl)furan-2-carbaldehyde: the method is as follows: mix 4.143 g of p-nitroaniline, 8 mL of concentrated hydrochloric acid and 16 mL of water and slowly heat to reflux until the nitroaniline is completely dissolved . After the dissolution is complete, place the round-bottomed flask in an ice bath while accelerating stirring to precipitate tiny crystals. Weigh 6 grams of NaNO 2 Dissolve it in 9mL water, slowly add it dropwise into the aniline solution with a constant pressure funnel, stir and react for 20 minutes after dropping, filter, transfer the filtrate to a 250mL round-bottomed flask, add 2.9g of furfuraldehyde, 20mL of acetone and 40 Milliliter of water, stir under ice bath, dissolve 0.8 g of copper chloride in 3 mL of water, slowly add it dropwise, remove the ice bath after dripping, continue to react at room temperature for 8 hours, a brick red precipitate is formed, filter, us...

Embodiment 2

[0047] 1. Synthesis of receptor compounds

[0048] (1) Synthesis of intermediate 5-(nitrophenyl)furan-2-carbaldehyde: same as in Example 1.

[0049] (2) Synthesis of acceptor compound: Add about 1.1g (5mmol) of 5-(nitrophenyl)furan-2-carbaldehyde and about 0.8g (5.5mmol) of α-naphthylamine into a 50mL round bottom flask, Dissolve in 30mL of hot EtOH, and add 1mL of AcOH as a catalyst, then reflux at 85°C for 4h, cool to room temperature, filter the brown precipitate with suction, wash the precipitate with hot EtOH three times, and finally use DMF / EtOH (1:1 / v: v) The solution was recrystallized to obtain a brownish-yellow solid, which was the acceptor compound (4.30 mmol), and the yield was 86.7%.

[0050] 2. Hg 2+ Preparation and detection of test paper

[0051] (1) Hg 2+ Preparation of detection test paper: the concentration of acceptor compound DMSO solution is 1.5×10 -3 mol L -1 Others are with embodiment 1.

[0052] (2) Test paper to detect Hg 2+ : with embodiment ...

Embodiment 3

[0054] 1. Synthesis of receptor compounds

[0055] (1) Synthesis of intermediate 5-(nitrophenyl)furan-2-carbaldehyde: same as in Example 1.

[0056] (2) Synthesis of acceptor compounds: Add about 1.1g (5mmol) of 5-(nitrophenyl)furan-2-carbaldehyde and about 1.0g (7.25mmol) of α-naphthylamine into a 50mL round bottom flask, dissolve in In 30mL hot EtOH, add 1mLAcOH as a catalyst, then reflux at 85°C for 4h, after cooling to room temperature, filter the brown precipitate with suction, wash the precipitate with hot EtOH three times, and finally recrystallize with DMF / EtOH solution to obtain a brown solid , which is the acceptor compound (ATS) (4.2mmol), yield 85.2%.

[0057] 2. Hg 2+ Preparation and detection of test paper

[0058] (1) Hg 2+ Preparation of detection test paper: the concentration of acceptor compound DMSO solution is 2.0×10 -3 mol L - 1. Others are the same as in Embodiment 1.

[0059] (2) Test paper to detect Hg 2+ : with embodiment 1.

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Abstract

The invention provides a receptor compound for identifying mercury ions by virtue of colorimetry-fluorometry dual channels and belongs to the technical field of cation detection. The preparation method of the receptor compound comprises the steps of carrying out reflux reaction on 5-(nitrophenyl)furan-2-formaldehyde and alpha-naphthylamine in the presence of ethanol as a solvent and acetic acid as a catalyst, precipitating, carrying out suction filtration, washing with ethanol and recrystallizing with a DMF / EtOH solution. By colorimetry and fluorescent spectrometry, the identification effects of the receptor compound on eleven kinds of cations, namely, Fe<3+>, Hg<2+>, Ca<2+>, Cu<2+>, Co<2+>, Ni<2+>, Cd<2+>, Pb<2+>, Zn<2+>, Cr<3+>, Mg<2+>, are detected, the detection results show that the receptor compound has high sensitivity and single selective colorimetric and fluorescent identification capabilities on Hg<2+> ion in the pure DMSO (dimethylsulfoxide). Furthermore, a piece of mercury ion detection test paper based on the receptor is also prepared, and by virtue of the detection test paper, mercury ions can be conveniently subjected to colorimetric-fluorescent detection, and thus the mercury ion detection test paper good prospects in detecting mercury ions.

Description

technical field [0001] The invention belongs to the technical field of cation detection, and relates to a mercury ion acceptor compound; in particular, it relates to an acceptor compound capable of identifying mercury ions through colorimetric-fluorescence dual channels. The invention also relates to the preparation of the mercury ion acceptor compound and its application in the colorimetric-fluorescent dual-channel identification of mercury ions. Background technique [0002] The heavy metal mercury is a highly toxic substance that pollutes the environment for a long time. Mercury pollution has become a major global environmental problem. my country is a large country in the production, use and emission of mercury, and the situation of mercury pollution prevention and control is very severe. Mercury analysis and monitoring technology is the basis of mercury pollution prevention and control. At present, most of the mature mercury detection technologies rely on large-scale ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/52C09K11/06G01N21/64G01N21/78
CPCC07D307/52C09K11/06C09K2211/1088G01N21/643G01N21/78G01N2021/755
Inventor 张有明曲文娟高国莹史兵兵魏太保
Owner NORTHWEST NORMAL UNIVERSITY
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